Journal of Dairy Science and Technology ›› 2023, Vol. 46 ›› Issue (1): 24-29.DOI: 10.7506/rykxyjs1671-5187-20221107-066

• Analysis & Detection • Previous Articles     Next Articles

Determination of Ethylene Oxide and 2-Chloroethanol in Milk and Dairy Products

ZHOU Jing, XU Hongbin, ZHOU Zelin, ZHOU Yaobin, FU Changyu, LIU Yang   

  1. Key Laboratory of Milk and Dairy Products Detection and Monitoring Technology for State Market Regulation, Shanghai Institute of Quality Inspection and Technical Research, Shanghai 200233, China
  • Online:2023-01-01 Published:2023-03-21

乳及乳制品中环氧乙烷及2-氯乙醇的检测

周 静,徐红斌,周泽琳,周耀斌,符昌雨,刘 洋   

  1. 上海市质量监督检验技术研究院,国家市场监管重点实验室(乳及乳制品检测与监控技术),上海 200233

Abstract: In this study, headspace gas chromatography-mass spectrometry (HS-GC-MS) was used to accurately identify and quantify ethylene oxide and 2-chloroethanol in milk and dairy products (liquid milk, fermented milk, infant formula milk powder, and ice cream). The sample was diluted to a constant volume in a headspace bottle and balanced at 90 ℃ for 20 min, and the extract was separated on a DB-624 capillary column (60 m × 0.32 mm, 1.8 μm) with temperature programming. Ethylene oxide and 2-chloroethanol were detected using an electrospray ionization (ESI) source in the selected ion monitoring (SIM) mode. Quantitation was carried out using matrix-matched calibration curves. Good linearity was obtained in the range of 0.1–10.0 mg/L (R2 ≥ 0.99). The limits of detection of ethylene oxide and 2-chloropropanol in milk, fermented milk and ice cream were 0.12 and 0.60 mg/kg, respectively. At three spiked levels, the average recoveries of the two compounds were between 75.9% and 101.6%, with relative standard deviations (RSD) less than 10%. This method is precise and accurate, and can meet the requirements for the detection of milk and dairy products with a complex matrix.

Key words: ethylene oxide; 2-chloroethanol; milk and dairy products; headspace-gas chromatography-mass spectrometry

摘要: 采用顶空-气相色谱-质谱联用技术,实现对乳及乳制品(液态乳、发酵乳、婴幼儿配方乳粉、冰淇淋)中环氧乙烷和2-氯乙醇的准确定性和定量。样品于顶空瓶中经稀释定容后,90 ℃下平衡20 min,采用DB-624毛细管色谱柱(60 m×0.32 mm,1.8 μm)程序升温模式实现目标物色谱分离,质谱采用选择离子扫描模式对环氧乙烷和2-氯乙醇进行检测,基质匹配标准曲线法定量。结果表明:该方法在0.1~10.0 mg/L线性良好(R2≥0.99),环氧乙烷和2-氯乙醇在液态乳、发酵乳和冰淇淋中的检出限为0.12、0.60 mg/kg;在低、中、高3 个加标水平下,2 种化合物的平均回收率为75.9%~101.6%,相对标准偏差均小于10%。该方法精密度和准确度良好,且方法灵敏度高,满足乳及乳制品复杂基质中环氧乙烷和2-氯乙醇的检测要求。

关键词: 环氧乙烷;2-氯乙醇;乳及乳制品;顶空-气相色谱-质谱联用

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